Calcium Gluconate Tablets DEFINITION Calcium Gluconate Tablets contain NLT 95.0% and NMT 105.0% of the labeled amount of calcium gluconate (C12H22CaO14). IDENTIFICATION • A. Identification TestsGeneral, Calcium 191 Sample stock solution: A warm, filtered solution in water, equivalent to 100 mg/mL of calcium gluconate from powdered Tablets Sample solution: Equivalent to 20 mg/mL of calcium gluconate from a dilution of the Sample stock solution Acceptance criteria: Meet the requirements • B. Thin-Layer Chromatographic Identification Test Standard solution: 10 mg/mL of USP Potassium Gluconate RS Sample solution: Equivalent to 10 mg/mL of calcium gluconate from a dilution of the Sample stock solution obtained from Identification test A Chromatographic system Adsorbent: 0.25-mm layer of chromatographic silica gel Application volume: 5 µL Developing solvent system: Alcohol, ethyl acetate, ammonium hydroxide, and water (50:10:10:30) Spray reagent: Dissolve 2.5 g of ammonium molybdate in 50 mL of 2 N sulfuric acid in a 100-mL volumetric flask, add 1.0 g of ceric sulfate, swirl to dissolve, and dilute with 2 N sulfuric acid to volume. Analysis Samples: Standard solution and Sample solution Develop until the solvent front has moved about three-fourths of the length of the plate. Remove the plate, and dry at 110 for 20 min. Allow to cool, and spray with Spray reagent. Heat the plate at 110 for about 10 min. Acceptance criteria: The principal spot of the Sample solution corresponds in color, size, and RF value to that of the Standard solution. ASSAY • Procedure Sample: A portion of the powder from NLT 20 finely powdered Tablets, equivalent to 500 mg of calcium gluconate Blank: Proceed as directed in the Analysis, without the Sample. Titrimetric system (See Titrimetry 541.) Mode: Direct titration Titrant: 0.05 M edetate disodium VS Indicator: Hydroxy naphthol blue, 300 mg Endpoint detection: Visual Analysis: Transfer the Sample to a suitable crucible. Ignite, gently at first, until free from carbon. Cool the crucible. Add 10 mL of water, and dissolve the residue by adding sufficient 3 N hydrochloric acid, dropwise, to achieve complete solution. Transfer the solution to a suitable container, and add about 150 mL of water. While stirring, preferably with a magnetic stirrer, add 20 mL of Titrant from a 50-mL buret. Add 15 mL of 1 N sodium hydroxide, then add the Indicator. Continue the titration to a blue endpoint. Perform a Blank determination. Calculate the percentage of the labeled amount of calcium gluconate (C12H22CaO14) in the portion of Tablets taken: Result = {[(VS VB) × M × F]/W} × 100
Acceptance criteria: 95.0%105.0% PERFORMANCE TESTS • Dissolution 711 Medium: Water; 900 mL Apparatus 2: 50 rpm Time: 45 min Standard solution: Solution having a known concentration of calcium in Medium Sample solution: Filtered portion of the solution under test, suitably diluted with Medium if necessary Instrumental conditions Mode: Atomic absorption spectrophotometry Analytical wavelength: 422.8 nm Lamp: Calcium hollow-cathode Flame: Airacetylene Analysis Samples: Standard solution and Sample solution Calculate the percentage of the labeled amount of calcium gluconate (C12H22CaO14) dissolved: Result = (AU/AS) × (CS × D × V/L) × (Mr/Ar) × 100
Tolerances: NLT 75% (Q) of the labeled amount of calcium gluconate (C12H22CaO14) is dissolved. • Uniformity of Dosage Units 905: Meet the requirements ADDITIONAL REQUIREMENTS • Packaging and Storage: Preserve in well-closed containers. Auxiliary Information Please check for your question in the FAQs before contacting USP.
USP35NF30 Page 2456 Pharmacopeial Forum: Volume No. 27(6) Page 3258 |